US6383285B1 - Method for producing crystalline silicon - Google Patents

Method for producing crystalline silicon Download PDF

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Publication number
US6383285B1
US6383285B1 US09/551,568 US55156800A US6383285B1 US 6383285 B1 US6383285 B1 US 6383285B1 US 55156800 A US55156800 A US 55156800A US 6383285 B1 US6383285 B1 US 6383285B1
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United States
Prior art keywords
molten silicon
silicon
inert gas
gas
lance
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US09/551,568
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English (en)
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Saburo Wakita
Yoshinobu Nakada
Junichi Sasaki
Yuji Ishiwari
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Mitsubishi Materials Corp
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Mitsubishi Materials Corp
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Assigned to MITSUBISHI MATERIALS CORPORATION reassignment MITSUBISHI MATERIALS CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: NAKADA, YOSHINOBU, ISHIWARI, YUJI, SASAKI, JUNICHI, WAKITA, SABURO
Priority to US10/103,797 priority Critical patent/US6540828B2/en
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/007—Mechanisms for moving either the charge or the heater
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/90—Apparatus characterized by composition or treatment thereof, e.g. surface finish, surface coating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y10T117/1016—Apparatus with means for treating single-crystal [e.g., heat treating]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y10T117/1024—Apparatus for crystallization from liquid or supercritical state

Definitions

  • the present invention is a method of producing crystalline silicon by cooling and solidifying molten silicon gradually in a unidirectional manner.
  • Polycrystalline silicon solar cells are the type of solar cells which are presently produced in the largest quantity.
  • the performance of a polycrystalline silicon solar cell element depends greatly on the quality of the polycrystalline silicon. For this reason, various improvements have been made in methods for producing polycrystalline silicon, particularly in methods to decrease the level of impurities and to improve the crystallinity of the polycrystalline silicon
  • Methods for producing polycrystalline silicon are roughly divided into two steps: a step in which high-purity silicon is produced from metallic silicon, and a step of solidifying molten high-purity silicon by a unidirectional solidification process.
  • metallic silicon is reacted with hydrochloric acid to obtain gaseous trichlorosilane, followed by rectifying the gaseous trichlorosilane and then precipitating high-purity silicon from the gas while reducing the rectified gas with hydrogen gas, thereby forming high-purity silicon.
  • the level of impurities in the silicon may also be reduced by stirring the molten silicon during the unidirectional solidification step.
  • JP-A 61-141612 discloses a method of turning a mold containing the molten silicon
  • JP-A 5-254817 discloses a method of stirring molten silicon by means of a magnetic field
  • JP-A 10-182135 discloses a method which comprises blowing an inert gas into the molten silicon by inserting a gas-supplying lance into the molten silicon above the solid-liquid phase boundary between the molten and solid silicon.
  • the above-mentioned first method requires expensive equipment, has a high production cost, and requires difficult and costly equipment maintenance.
  • the second method requires expensive equipment.
  • the third method has the problem that the gas-supplying lance tends to melt and deposit impurities into the molten silicon, resulting in less pure silicon.
  • the properties of solar cells made from silicon having a high oxygen content are poorer than those of solar cells made from silicon having a lower oxygen content.
  • a certain level of oxygen is dissolved or otherwise incorporated into remelted, lump silicon derived from single crystal silicon scrap, which is a convenient main raw material. It is therefore necessary to decrease the oxygen level in the silicon during the process of melting and unidirectional solidification.
  • a carbon oxide gas (CO), silicon oxide gas (SiO) and the like are absorbed into the molten silicon, thereby increasing the level of carbon and oxygen impurities therein, which results in a degradation of the properties of the resulting solar cells.
  • carbon oxide gas includes any gaseous oxide of carbon, for example carbon monoxide or carbon dioxide, or mixtures thereof
  • silicon oxide gas includes any oxide of silicon, for example, silicon dioxide.
  • the present invention is a method for producing high quality polycrystalline silicon at a low cost, which has low impurity levels and high crystallinity.
  • the following aspects of the present invention further describe the present invention:
  • the first aspect of the present invention is a process for producing crystalline silicon in which molten silicon crystallizes upward from the inner bottom of a mold by means of a positive temperature gradient extending from the inner bottom of the mold upward, in which the temperature of the silicon increases from the bottom of the mold, upward.
  • an inert gas such as argon (Ar) is blown onto the surface of the molten silicon from a position above the surface of the molten silicon, in order to vibrate the surface of the molten silicon in such a manner that cavities are formed in the surface.
  • the vibration continuously forms a fresh surface on the molten silicon which promotes the discharge to the surrounding atmosphere of SiO gas generated in the interior of the molten silicon, which is effective in removing oxygen (O) impurities in the molten silicon.
  • a gas-supplying lance is not inserted into the molten silicon, there is less chance of contaminating the molten silicon with impurities derived from the gas-supplying lance.
  • the second aspect of the present invention is a process for producing crystalline silicon as mentioned in (1), in which the surface of the molten silicon is covered with an inert gas.
  • an inert gas such as Ar
  • contaminating gases such as CO gas and SiO gas from the surrounding atmosphere are not absorbed by the molten silicon.
  • the third aspect of the present invention is a process for producing crystalline silicon as mentioned in (1) or (2), in which a susceptor is located above the surface of the molten silicon and the inert gas is introduced into the space between the susceptor and molten silicon through an opening in the susceptor.
  • the inert gas present near the surface of the molten silicon is restrained from diffusing into the surrounding atmosphere by the susceptor, so the inert gas can cover the surface of the molten silicon for a long time. Therefore, the CO gas and SiO gas in the surrounding atmosphere are effectively prevented from entering into the molten silicon by a small flow rate of an inert gas.
  • the fourth aspect of the present invention is a process for producing crystalline silicon as mentioned in any one of (1) to (3), in which the flow rate of the inert gas blown into the mold is reduced as the solid-liquid phase boundary of the silicon in the mold moves upward. This prevents the solid -liquid phase boundary from being disturbed by the blown inert gas.
  • the fifth aspect of the present invention is a process for producing crystalline silicon as mentioned in any one of (1) to (4), in which the flow rate of the inert gas blown into the mold, the inside radius of the gas-supplying lance which introduces the inert gas onto the surface of the molten silicon, and the distance from a nozzle of the lance to the surface of the molten silicon satisfy the following formula;
  • f in units of 1/min is the flow rate of the inert gas
  • r in units of cm is the inside radius of the lance
  • H in units of cm is the distance from a port of the lance to the surface of molten silicon.
  • the flow rate of the blown gas, the inside radius of the gas-supplying lance and the distance from a port of the lance to the surface of the molten silicon are conditions selected so that the surface of the molten silicon is vibrated effectively, promoting the discharge to the surrounding atmosphere of SiO gas generated in the interior of the molten silicon. Therefore, the level of O impurities in the molten silicon can be reduced.
  • the sixth aspect of the present invention is a process for producing crystalline silicon as mentioned in any one of (1) to (5), in which there are one or more gas nozzles on the lance, and the number of nozzles increases as the surface area of the molten silicon increases.
  • the surface of the molten silicon is vibrated by the lance nozzles, the number of which is selected according to the surface area of the molten silicon, so as to effectively promote the discharge to the surrounding atmosphere of SiO gas generated in the interior of the molten silicon. This causes a reduction in the O impurity level in the molten silicon.
  • FIG. 1 is a schematic sectional view showing an apparatus consisting of a mold, heaters, a cooling plate, a susceptor, and thermal insulation which is used for producing crystalline silicon according to the present invention.
  • FIG. 2 is a plan view of FIG. 1, viewed from the perspective of a gas-supplying lance, and which illustrates the inert gas flow.
  • FIGS. 3 ( a ) and ( b ) show the relation between the rate of inert gas flow and the position of the solid-liquid phase boundary.
  • FIG. 4 ( a ) is a schematic sectional view of another example of a mold and a susceptor for producing crystalline silicon according to the present invention.
  • FIG. 4 ( b ) is a plan view of FIG. 4 ( a ) which illustrates the inert gas flow.
  • the entire apparatus illustrated in FIG. 1 is located within a large chamber, not shown in the drawing.
  • a solid silicon raw material is charged into mold 1 .
  • an inert gas atmosphere is introduced from the upper part of the chamber holding the apparatus of FIG. 1 .
  • the solid silicon in the mold is then heated by the upper heater 2 a and lower heater 2 b to melt the solid silicon, providing molten silicon 10 .
  • an inert gas for example Ar gas, supplied from the gas-supplying lance 5 , covers the surface of the molten silicon.
  • the flow pattern of the inert gas is illustrated by the arrow symbols in FIG. 2 .
  • the inert gas provided by the lance vibrates the surface of the molten silicon so that cavities are formed in the molten silicon surface.
  • a positive temperature gradient is a temperature gradient in which the temperature of the mold and the silicon therein increases from the bottom to the top of the mold.
  • the surface of the molten silicon vibrates so that a fresh surface is continually formed in the surface of the molten silicon.
  • the contamination of the molten silicon by CO gas from the surrounding atmosphere is prevented by this flow of inert gas.
  • an ingot of crystalline silicon having a low level of impurities such as C and O is obtained.
  • this crystalline silicone has excellent crystallinity.
  • crystalline silicon is obtained at a low cost, as it is sufficient that the lance is positioned above the mold so as to blow the inert gas onto the surface of the molten silicon.
  • FIGS. 3 ( a ) and ( b ) shows the relationship between the flow rate of the inert gas and the position of the solid-liquid phase boundary, 11 .
  • the rate of flow of the inert gas directed out of the lance 5 , onto the molten silicon, 10 b is high.
  • the rate of inert gas flow out of the lance is reduced, so as not to disturb the solid-liquid phase boundary.
  • FIG. 4 illustrates a schematic of an alternative apparatus in which an oval or round susceptor 6 is placed directly on top of a square or rectangular mold 1 , so that the inert gas flow can escape through the opening between the mold and the susceptor.
  • any shape of mold and susceptor is acceptable as long as the inert gas from the lance can fill the space between the susceptor and the surface of the molten silicon, and the inert gas can flow out of the mold.
  • Ingots of crystalline silicon were produced using the above-described apparatus for producing crystalline silicon according to the present invention.
  • a quartz mold was used having a dimension of about 17 ⁇ 17 ⁇ 11 (cm).
  • Approximately 3 kg of scrap single crystal silicon used for semiconductors was used as the solid silicon raw material.
  • the silicon was heated up to 1500° C. in one hour, and the silicon was completely melted in 1.5 hours. After the silicon was completely melted, the required inert gas flow was begun. Ar gas atmosphere was used in the chamber.
  • the Ar gas was blown onto the surface of the molten silicon at various flow rates as follows: 2, 10, 40 and 60 l/min.
  • the gas flow rate was successively decreased as the solid-liquid phase boundary moved upward. Accordingly, the solid-liquid phase boundary was not disturbed with the result that crystalline silicon having excellent crystallinity was produced.
  • the height of the ingots obtained as described above were about 5 cm.
  • C and O contents were measured in the center of the face of a wafer obtained at a height of 2.0 cm from the bottom of each ingot.
  • the “a” superscript indicates that the conditions satisfied the relation 5.0 ⁇ f/(rH) ⁇ 25 and the superscript “b” indicates that the conditions satisfied the relation 3.0 ⁇ f/(rH) ⁇ 60.
  • the asterisk symbol “*” indicates conditions in which molten silicon splashed and sputtered to the upper heater.
  • the upper half of Table 1 shows the C impurity level and the lower half shows the O impurity level.
  • the numeral located on the left side of the slash “ ⁇ ” is the value of the impurity level, while the numeral located to the right of the slash “ ⁇ ” is the value of the relation f/(rH).
  • both the C and O impurity levels are high. In contrast, under conditions satisfying the relation 3 ⁇ f/(rH) ⁇ 5, the C and O impurity levels are lower. Under conditions satisfying the relation 5.0 ⁇ f/(rH) ⁇ 25, the C and O impurity levels decrease to approximately half that of silicon produced under conditions satisfying the relation 3>f/(rH). Under conditions satisfying the relation f/(rH)>25, although the C and O impurity levels decrease further, the crystallinity of the silicon was disturbed and the solar cell properties were reduced because it was difficult to control the process such that the solid-liquid phase boundary was not disturbed.
  • the C and O impurity levels of crystalline silicon prepared by the process of the present invention are lower than those of the comparative example when the process conditions satisfy the relation 3.0 ⁇ f/(rH) ⁇ 60.
  • the process conditions satisfy the relation 5.0 ⁇ f/(rH) ⁇ 25 the C and O impurity levels are greatly reduced.
  • the impurity levels increase. If r is larger than 3 cm, the impurity levels are the same as that of the comparative example.
  • the susceptor may have a diameter larger than the width of the opening of the mold and can be placed directly on top of the opening of the mold.
  • a plurality of lances may be used if the surface are of the molten silicon is large.
  • a small mold in which the surface area of the molten silicon is correspondingly small may only require only one gas-supplying lance to effectively vibrate the molten silicon surface, and thereby exhaust the SiO gas generated in the interior of the molten silicon.
  • Larger molds, in which the surface area of the molten silicon is correspondingly larger, may require two or more gas-supplying lances in order to prepare high-purity silicon according to the present invention.
  • the first aspect of the present invention is a process for producing crystalline silicon which has low impurity levels and excellent crystallinity, since the solidification and crystallization of the silicon are carried out while simultaneously removing O impurities from the molten silicon by promoting the discharge to the surrounding atmosphere of SiO gas which was generated in the interior of the molten silicon during the crystallization.
  • the second aspect of the present invention is a process for producing a crystalline silicon, in which impurity gases such as CO gas and SiO gas from the surrounding atmosphere are prevented from being absorbed by the molten silicon.
  • the third aspect of the present invention is a process for producing crystalline silicon, in which CO gas and SiO gas from the surrounding atmosphere are effectively prevented from being absorbed by the molten silicon by providing a small flow rate of an inert gas over the surface of the molten silicon.
  • the fourth aspect of the present invention is a process for producing crystalline silicon, in which the solid-liquid phase boundary is not disturbed by by reducing the flow rate of the inert gas as crystallization proceeds, with the result that a crystalline silicon having an excellent crystallinity is obtained.
  • the fifth aspect of the present invention is a process for producing crystalline silicon having a greatly reduced level of O impurities which is produced by vibrating the surface of the molten silicon by selecting a flow rate of the inert gas, the inside radius of the gas-supplying lance and the distance from a port of the lance to the surface of the molten silicon in order to promote the discharge to the surrounding atmosphere, of SiO gas generated in the interior of the molten silicon, thereby removing O impurities in the molten silicon.
  • the sixth aspect of the present invention is a process for producing crystalline silicon in which the level of O impurities can be reduced by vibrating the molten silicon by a number of lances, in which the number of lances employed depends on the surface area of the molten silicon, so that the SiO gas generated in the interior of the molten silicon is effectively discharged to the surrounding atmosphere.

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
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US09/551,568 1999-04-30 2000-04-18 Method for producing crystalline silicon Expired - Lifetime US6383285B1 (en)

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Applications Claiming Priority (4)

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JP12533999 1999-04-30
JP11-125339 1999-04-30
JP12-054820 2000-02-29
JP2000054820A JP3885452B2 (ja) 1999-04-30 2000-02-29 結晶シリコンの製造方法

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EP (1) EP1048758B1 (de)
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US20040050522A1 (en) * 2002-07-25 2004-03-18 Mitsubishi Materials Corporation Casting apparatus and method therefor
DE102005013410A1 (de) * 2005-03-23 2006-09-28 Deutsche Solar Ag Vorrichtung und Verfahren zum Kristallisieren von Nichteisenmetallen
US20070227189A1 (en) * 2004-03-29 2007-10-04 Kyocera Corporation Silicon Casting Apparatus and Method of Producing Silicon Ingot
US20070283882A1 (en) * 2006-06-13 2007-12-13 Young Sang Cho Manufacturing equipment for polysilicon ingot
US20080178793A1 (en) * 2007-01-31 2008-07-31 Calisolar, Inc. Method and system for forming a higher purity semiconductor ingot using low purity semiconductor feedstock
US20100127221A1 (en) * 2007-04-27 2010-05-27 Freiberger Compound Materials Gmbh Device and process for producing poly-crystalline or multi-crystalline silicon; ingot as well as wafer of poly-crystalline or multi-crystalline silicon produced thereby, and use for the manufacture of solar cells
US10112838B2 (en) 2013-09-02 2018-10-30 Commissariat A L'energie Atomique Et Aux Energies Alternatives Method and device for treating the free surface of a material
US11329284B2 (en) 2016-05-20 2022-05-10 Nano One Materials Corporation Fine and ultrafine powders and nanopowders of lithium metal oxides for battery applications

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US8268074B2 (en) * 2005-02-03 2012-09-18 Rec Scan Wafer As Method and device for producing oriented solidified blocks made of semi-conductor material
WO2007010622A1 (ja) * 2005-07-22 2007-01-25 Kyocera Corporation 多結晶シリコン基板及びその製造方法、並びに光電変換素子及び光電変換モジュール
TW200726812A (en) * 2005-11-25 2007-07-16 Hitachi Chemical Co Ltd Liquid resin composition for electronic components and electronic components device
FR2895749B1 (fr) * 2006-01-04 2008-05-02 Apollon Solar Soc Par Actions Dispositif et procede de fabrication d'un bloc de materiau cristallin
KR100853019B1 (ko) 2007-01-19 2008-08-19 주식회사 글로실 태양전지용 다결정 실리콘 주괴 제조 방법
CN101755075A (zh) * 2007-07-20 2010-06-23 Bp北美公司 从籽晶制造浇铸硅的方法和装置
TW200930850A (en) * 2008-01-03 2009-07-16 Green Energy Technology Inc Cooling structure for body of crystal growth furnace
DE112008003810A5 (de) * 2008-02-14 2011-01-20 Deutsche Solar Ag Vorrichtung und Verfahren zur Herstellung von kristallinen Körpern durch gerichtete Erstarrung
EP2334847B1 (de) 2008-09-19 2013-06-19 MEMC Singapore Pte. Ltd. Direktionaler erstarrungsofen und verfahren für verringerte schmelzekontaminierung und verringerte waferkontaminierung
EP2492242A4 (de) 2009-10-19 2015-07-22 Jx Nippon Mining & Metals Corp Ofen zum schmelzen von silicium oder siliciumlegierungen
JP5371701B2 (ja) * 2009-11-04 2013-12-18 三菱マテリアルテクノ株式会社 多結晶シリコンインゴットの製造装置及び多結晶シリコンインゴットの製造方法
JP5606976B2 (ja) * 2011-03-25 2014-10-15 三菱マテリアル株式会社 シリコンインゴット製造装置、シリコンインゴットの製造方法
JP6064596B2 (ja) * 2012-02-28 2017-01-25 三菱マテリアル株式会社 鋳造装置及び鋳造方法
KR101964999B1 (ko) * 2012-02-28 2019-04-02 미쓰비시 마테리알 가부시키가이샤 주조 장치 및 주조 방법
JP5979664B2 (ja) * 2012-07-30 2016-08-24 国立研究開発法人物質・材料研究機構 シリコン結晶鋳造炉
WO2021031140A1 (zh) * 2019-08-21 2021-02-25 眉山博雅新材料有限公司 开放式温场

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US6540828B2 (en) 2003-04-01
DE60015228D1 (de) 2004-12-02
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US20020139297A1 (en) 2002-10-03
EP1048758B1 (de) 2004-10-27

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